Separation of fullerene C 60 and C 70 using crystallization

Chemistry: physical processes – Physical processes – Crystallization

Reexamination Certificate

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C023S296000

Reexamination Certificate

active

07875086

ABSTRACT:
The present invention is a method for simultaneously separating two highly pure fullerenes from a mixture of fullerenes via crystallization, by (i) adjusting the amount of solvent in the mixture fed to a first crystallizer to obtain a phase equilibrium behavior so a first fullerene component of the two fullerenes, in the form of pure crystal, solid solution crystal, or solvate crystal is obtained; (ii) adjusting the amount of solvent in another mixture fed to a second crystallizer, operating at a temperature different from the first crystallizer, to obtain a phase equilibrium behavior so a second fullerene component of the two fullerenes, in the form of pure crystal, solid solution crystal, or solvate crystal is obtained; and additionally (iii) purifying the solid solution or the solvate into highly pure fullerene, when the solid product from the crystallizers is in the form of solid solution or solvate.

REFERENCES:
patent: 5188918 (1993-02-01), Ziolo
patent: 5711927 (1998-01-01), Atwood et al.
patent: 2004-244245 (2004-09-01), None
Atwood et al., “Purification of C60and C70by Selective Complexation with Calixarenes.”Nature, v.368 pp. 229-231 (1994).
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Taylor et al., “Isolation, Separation and Characterisation of the Fullerenes C60and C70: The Third Form of Carbon.”J. Chem. Soc., Chem. Commun., pp. 1423-1425 (1992).
Vassalio et al., “Improved Separation of Fullerene-60 and -70.”J. Chem. Soc., Chem. Commun., pp. 60-61 (1992).
Scrivens et al., “Purification of Gram Quantities of C60: A New Inexpensive and Facile Method.”J. Am. Chem. Soc., v.114 pp. 7917-7919 (1992).
Coustel et al., “Purification of C60by a Simple Crystallization Procedure.”J. Chem. Soc., Chem. Commun., pp. 1402-1403 (1992).
Rudy M. Baum, “Chemists Increasingly Adept at Modifying, Manipulating Fullerenes.”Chemical and Engineering News, pp. 31-33 (Sep. 20, 1993).
Zhou et al., “Seperation of C60and C70Fullerenes in Gram Quantities by Fractional Crystallization.”Carbon, v.32(5) pp. 935-937 (1994).

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